EP0797689B1 - Dispositif d'extraction de gaz - Google Patents

Dispositif d'extraction de gaz Download PDF

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Publication number
EP0797689B1
EP0797689B1 EP95941752A EP95941752A EP0797689B1 EP 0797689 B1 EP0797689 B1 EP 0797689B1 EP 95941752 A EP95941752 A EP 95941752A EP 95941752 A EP95941752 A EP 95941752A EP 0797689 B1 EP0797689 B1 EP 0797689B1
Authority
EP
European Patent Office
Prior art keywords
hydrolysis reactor
outlet
oven
pump
hydrolysis
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP95941752A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP0797689A1 (fr
Inventor
Jean-Luc Charvet
Stéphane Goujard
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Safran Aircraft Engines SAS
Original Assignee
Societe Nationale dEtude et de Construction de Moteurs dAviation SNECMA
SNECMA SAS
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Societe Nationale dEtude et de Construction de Moteurs dAviation SNECMA, SNECMA SAS filed Critical Societe Nationale dEtude et de Construction de Moteurs dAviation SNECMA
Publication of EP0797689A1 publication Critical patent/EP0797689A1/fr
Application granted granted Critical
Publication of EP0797689B1 publication Critical patent/EP0797689B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/4412—Details relating to the exhausts, e.g. pumps, filters, scrubbers, particle traps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/46—Removing components of defined structure
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S261/00—Gas and liquid contact apparatus
    • Y10S261/54—Venturi scrubbers

Definitions

  • the present invention relates to industrial installations of manufacture of composite material parts comprising infiltration ovens or chemical vapor deposition. More particularly, the subject of the invention is a gas extraction device for such installations.
  • a known technique for manufacturing parts made of materials composites in particular parts made of thermostructural composite materials, such as carbon-carbon composites or ceramic matrix composites, consists of making preforms of the parts and densifying the preforms in infiltration furnaces or chemical vapor deposition.
  • Part preforms are generally made up of fibrous textures.
  • Preforms, possibly kept in shape by tools, are introduced into a oven in which a gas phase is admitted, the composition of which is chosen according to of the nature of the matrix of the composite material.
  • the gaseous phase diffuses within the porosity of the preforms and, by decomposition of one of its constituents or reaction between several constituents, leaves a solid deposit which gradually densifies the preforms by filling their porosity, in order to form the matrix.
  • Gaseous reaction products and / or residues from the gas phase pumped out of the oven can cause problems due to their toxic or corrosive nature, or their tendency to form parasitic deposits.
  • a ceramic phase such as a silicon carbide (SiC for example), or even more particularly when the matrix comprises at least one phase consisting of a ceramic such as boron carbide (B 4 C) or a ternary silicon-boron-carbon system (Si-BC), as described in document FR-A-2 668 477.
  • SiC silicon carbide
  • Si-BC ternary silicon-boron-carbon system
  • the precursors used in the gas phase then usually comprise gaseous halides, in particular gaseous chlorides, which, in addition to their corrosive nature and their toxicity, can form significant solid deposits at the outlet of the oven. This is so, in particular with boron trichloride BCl 3 , precursor of the element boron.
  • the present invention aims to provide a device gas extraction which avoids the aforementioned drawbacks, in particular which avoids the formation of parasitic deposits which can cause blockages.
  • the current Another object of the invention is to provide an extraction device comprising means for treating corrosive and toxic gases from the oven, before discharge to the atmosphere.
  • a gas extraction device comprising a dry pump having an inlet connected to the oven to allow the establishment, the interior of the furnace, desired low pressure conditions, and gas extraction residual; and an atmospheric pressure hydrolysis reactor connected to an outlet of the pump is dry and intended to receive residual gases from the oven, the hydrolysis reactor comprising a first outlet for solid deposits or acid solutions from the hydrolysis of the gases received and a second outlet from gas connected to the atmosphere.
  • means are provided for injecting a gas, preferably a neutral gas, such as nitrogen, between the inlet of the dry pump and the inlet of the hydrolysis reactor.
  • a gas preferably a neutral gas, such as nitrogen
  • the gas injection can be carried out both at the inlet of the dry pump and in a pipe connecting the dry pump to the reactor hydrolysis.
  • this injection of gas contributes to oppose a counter current between the hydrolysis reactor and the pump and thus avoid the ascent to the pump of reaction products hydrolysis.
  • Water supply means are advantageously provided for establish a continuous liquid circulation between at least one access to the reactor hydrolysis and the first exit from it.
  • the water supply means are connected to the reactor hydrolysis at least through the second outlet thereof, in order to be able dissolve acid vapors from the reactor and avoid their rejection in the atmosphere.
  • the water supply means can be connected to a water injection inlet in a column connected to the second outlet of the reactor.
  • the first outlet of the hydrolysis reactor is connected to a neutralization tank in order to neutralize acid solutions produced by hydrolysis.
  • the illustrated gas extraction device is connected to the outlet of an oven 10 chemical vapor infiltration for example as described in document WO 87/04733 already cited.
  • the oven 10 comprises a reaction chamber 11 delimited by a graphite armature 12.
  • the armature is surrounded by a metal inductor 13 with the interposition of a thermal insulator 14.
  • the assembly is housed inside a sealed metal enclosure 15.
  • the armature 12 has the shape of a cylinder of vertical axis closed at its part lower by a bottom 12a and at its upper part by a removable cover 12b.
  • the preforms to be densified are placed on a tray perforated 16.
  • the preforms are for example structures fibrous having a shape close to that of parts to be made of material composite, possibly held in a tool.
  • the plate 16 can rotate around a vertical axis coincident with that of chamber 11. The rotation is controlled by a motor (not shown) coupled to the plate by a shaft 17 crossing the bottom 12a.
  • a reaction gas phase containing the precursor (s) of the matrix of composite material from reserves (not shown) is introduced into the chamber 11 by a supply pipe 18 which passes through enclosure 15 and leads to the upper part of the chamber through the cover 12b.
  • An additional flow of neutral gas for example nitrogen, can be added to the reaction gas phase to adjust the pressure in the bedroom.
  • the reaction gas phase entering the chamber 12 is forced to circulate in contact with preheating plates. These, formed of plates superimposed perforated 19, allow to quickly carry the gas phase reaction at the temperature prevailing in the chamber.
  • the extraction of the residual gas phase is carried out through one or more several pipes 20 which are connected to the lower part of the chamber 11 by an annular passage 21 surrounding the shaft 17.
  • the volume located around the armature 12 inside the enclosure 11 is continuously swept by a neutral gas, such as nitrogen. This is brought by a pipe 22. It is extracted from the enclosure 15 by a pipe 24. A neutral gas buffer is thus formed around the chamber 11.
  • a neutral gas such as nitrogen
  • a control unit receives signals produced by sensors and representative of the temperature and pressure in the chamber 11 and controls a generator 28 which supplies the current supply the inductor so as to maintain the temperature in the chamber at the predetermined optimal value for the infiltration operation chemical vapor phase.
  • the densification of the preforms contained in the infiltration furnace by a ceramic matrix in particular a matrix formed at least partially from the ternary system Si-BC, including SiC, B 4 C and SiB 4 , use of precursors in the gas phase consisting of toxic, corrosive gases capable of forming parasitic deposits at the outlet of the oven 10.
  • precursor gases are in particular gaseous chlorides such as Si x H y Cl z or B t H u Cl v (x, y, z, t, u and v being whole numbers).
  • the extraction gases outside the oven is carried out by means of a dry pump 32 connected to the oven 10 by line 30 and controlled by the installation control unit.
  • dry pump here we mean a pump which, for its operation, does not use no liquid, such as oil or water, capable of reacting with the gases from the oven to form parasitic deposits.
  • This pump also offers the advantage of having an operating temperature adjustable up to 160 ° C, allowing to choose a temperature of operation avoiding any phenomenon of recondensation in the body of the pump.
  • a filter 34 can be mounted in the pipe 30 to retain the solid particles having a dimension greater than a limit of preferably between 10 and 15 microns.
  • the filter 34 is for example constituted by a fine mesh of stainless steel, rolled up on itself, such as the effect filter cyclonic I.T.F. marketed by Edwards.
  • Means for treating the gases extracted by the pump are provided in downstream of the latter in order to avoid the release of toxic and corrosive gases into the atmosphere and the formation of parasitic deposits at the pump outlet.
  • the treatment means include a hydrolysis reactor 50 operating at atmospheric pressure and connected to the outlet of pump 32 by a line 40.
  • the gases from the pump reach the reactor along a path ascending, through a first part 42 of the pipe 40, then, following a downward path, first through a gas jet venturi 43, then through a tube 44 into which a helical part is inserted and which forms the vertical part end of the pipe 40.
  • the tube 44 ends at the upper part of the tank hydrolysis 50, through a cover 50a.
  • Acid solutions and solid deposits produced by the hydrolysis of gases residuals extracted by the pump are evacuated through an outlet 52, opening in the bottom 50b of the hydrolysis reactor.
  • the output 52 is connected to a neutralization tank 60 by means of a pipe 62.
  • the tank 60 contains a bath 64 suitable for neutralize the acid solutions brought to it via line 62.
  • a neutral gas for example nitrogen, is injected into the gas circuit extracts from the oven, on the one hand, at the inlet of the pump 32, through a pipe 46 and, on the other hand, in part 42 of the connection between the pump and the hydrolysis reactor, upstream of the venturi 43, by a pipe 48.
  • the injection of nitrogen has the effect of diluting the gases at the inlet of the pump 32 and to oppose an ascent to the acid vapor pump or solid particles from the hydrolysis reactor 50, thus preventing clogging of the pump vent.
  • the venturi 43 and the tube 44 of the pipe part 42 leading to the hydrolysis reactor and the downward direction of the gases in the tube 44 reinforce the interface function between the pump 32 and the hydrolysis reactor 50 which is ensured by the injection of nitrogen.
  • the hydrolysis reactor 50 has a gas outlet 54 communicating with the atmosphere through a tray column 70.
  • a filter 72 for example constituted by "Rashig" rings is inserted in column 70.
  • An injection inlet of water 74 is provided in column 70, at the top of it, and communicates with a water reserve (not shown) via a pipe 76.
  • the water thus injected forms a mist in the column and enters the reactor hydrolysis 50 through the outlet 54 forming a curtain of water 56.
  • the infiltration oven 10 is supplied with a gaseous phase containing gases which are precursors of SiC or of a ternary system Si-BC or of B 4 C
  • the gaseous chlorides Si x H y Cl z or B t H u Cl v are transformed in the hydrolysis reactor into a hydrochloric acid solution and into solid oxides SiO 2 and B 2 O 3 with release of hydrogen.
  • the gaseous species discharged into the atmosphere at the top of the column 70 are then constituted practically by hydrogen gas and the nitrogen injected into the extraction device.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Analytical Chemistry (AREA)
  • Biomedical Technology (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Health & Medical Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Vapour Deposition (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Feeding, Discharge, Calcimining, Fusing, And Gas-Generation Devices (AREA)
EP95941752A 1994-12-05 1995-12-01 Dispositif d'extraction de gaz Expired - Lifetime EP0797689B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
FR9414584A FR2727692A1 (fr) 1994-12-05 1994-12-05 Dispositif d'extraction de gaz pour four d'infiltration ou depot chimique en phase vapeur dans une installation de fabrication de pieces en materiau composite
FR9414584 1994-12-05
PCT/FR1995/001587 WO1996017972A1 (fr) 1994-12-05 1995-12-01 Dispositif d'extraction de gaz

Publications (2)

Publication Number Publication Date
EP0797689A1 EP0797689A1 (fr) 1997-10-01
EP0797689B1 true EP0797689B1 (fr) 1998-09-16

Family

ID=9469472

Family Applications (1)

Application Number Title Priority Date Filing Date
EP95941752A Expired - Lifetime EP0797689B1 (fr) 1994-12-05 1995-12-01 Dispositif d'extraction de gaz

Country Status (9)

Country Link
US (1) US6051071A (enrdf_load_stackoverflow)
EP (1) EP0797689B1 (enrdf_load_stackoverflow)
JP (1) JP3979663B2 (enrdf_load_stackoverflow)
CA (1) CA2206464C (enrdf_load_stackoverflow)
DE (1) DE69504868T2 (enrdf_load_stackoverflow)
ES (1) ES2124033T3 (enrdf_load_stackoverflow)
FR (1) FR2727692A1 (enrdf_load_stackoverflow)
GB (1) GB2295831B (enrdf_load_stackoverflow)
WO (1) WO1996017972A1 (enrdf_load_stackoverflow)

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US20030092174A1 (en) * 2001-05-14 2003-05-15 Monika Liljedahl Tissues or organs for use in xenotransplantation
US20030153044A1 (en) * 2001-05-14 2003-08-14 Monika Liljedahl Tissues or organs for use in xenotransplantation
US6702744B2 (en) * 2001-06-20 2004-03-09 Advanced Cardiovascular Systems, Inc. Agents that stimulate therapeutic angiogenesis and techniques and devices that enable their delivery
US8608661B1 (en) 2001-11-30 2013-12-17 Advanced Cardiovascular Systems, Inc. Method for intravascular delivery of a treatment agent beyond a blood vessel wall
US6953605B2 (en) * 2001-12-26 2005-10-11 Messier-Bugatti Method for densifying porous substrates by chemical vapour infiltration with preheated gas
US7361368B2 (en) 2002-06-28 2008-04-22 Advanced Cardiovascular Systems, Inc. Device and method for combining a treatment agent and a gel
US8383158B2 (en) * 2003-04-15 2013-02-26 Abbott Cardiovascular Systems Inc. Methods and compositions to treat myocardial conditions
US8821473B2 (en) 2003-04-15 2014-09-02 Abbott Cardiovascular Systems Inc. Methods and compositions to treat myocardial conditions
US8038991B1 (en) 2003-04-15 2011-10-18 Abbott Cardiovascular Systems Inc. High-viscosity hyaluronic acid compositions to treat myocardial conditions
US9539410B2 (en) 2005-04-19 2017-01-10 Abbott Cardiovascular Systems Inc. Methods and compositions for treating post-cardial infarction damage
US8828433B2 (en) 2005-04-19 2014-09-09 Advanced Cardiovascular Systems, Inc. Hydrogel bioscaffoldings and biomedical device coatings
US20080125745A1 (en) * 2005-04-19 2008-05-29 Shubhayu Basu Methods and compositions for treating post-cardial infarction damage
US8303972B2 (en) * 2005-04-19 2012-11-06 Advanced Cardiovascular Systems, Inc. Hydrogel bioscaffoldings and biomedical device coatings
US8187621B2 (en) * 2005-04-19 2012-05-29 Advanced Cardiovascular Systems, Inc. Methods and compositions for treating post-myocardial infarction damage
US7732190B2 (en) * 2006-07-31 2010-06-08 Advanced Cardiovascular Systems, Inc. Modified two-component gelation systems, methods of use and methods of manufacture
US9242005B1 (en) 2006-08-21 2016-01-26 Abbott Cardiovascular Systems Inc. Pro-healing agent formulation compositions, methods and treatments
US8741326B2 (en) * 2006-11-17 2014-06-03 Abbott Cardiovascular Systems Inc. Modified two-component gelation systems, methods of use and methods of manufacture
US9005672B2 (en) 2006-11-17 2015-04-14 Abbott Cardiovascular Systems Inc. Methods of modifying myocardial infarction expansion
US8192760B2 (en) 2006-12-04 2012-06-05 Abbott Cardiovascular Systems Inc. Methods and compositions for treating tissue using silk proteins
US10648075B2 (en) * 2015-03-23 2020-05-12 Goodrich Corporation Systems and methods for chemical vapor infiltration and densification of porous substrates
FR3114329B1 (fr) * 2020-09-24 2023-06-23 Safran Ceram Procédé de traitement d’une phase gazeuse résiduelle issue d’une technique CVI

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Also Published As

Publication number Publication date
JPH10509767A (ja) 1998-09-22
DE69504868T2 (de) 1999-05-20
GB9519431D0 (en) 1995-11-22
GB2295831B (en) 1998-04-29
DE69504868D1 (de) 1998-10-22
US6051071A (en) 2000-04-18
ES2124033T3 (es) 1999-01-16
JP3979663B2 (ja) 2007-09-19
FR2727692A1 (fr) 1996-06-07
WO1996017972A1 (fr) 1996-06-13
CA2206464A1 (en) 1996-06-13
CA2206464C (en) 2003-09-16
FR2727692B1 (enrdf_load_stackoverflow) 1997-02-28
GB2295831A (en) 1996-06-12
EP0797689A1 (fr) 1997-10-01

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